基于标准物质的卤素漏率量值复现方法研究

黄梓宸; 尹强; 叶丽芳; 贾相锐; 陈玲; 周军红

doi:10.12338/j.issn.2096-9015.2024.0264

基于标准物质的卤素漏率量值复现方法研究

doi: 10.12338/j.issn.2096-9015.2024.0264

黄梓宸^{1, 2,},
尹强¹,
叶丽芳¹,
贾相锐¹,
陈玲^{1, 2},
周军红^{1, 2}

1.
广东省计量科学研究院，广州 510405
2.
国家碳计量中心（广东），广州 510405）

基金项目: 广东省市场监督管理局科技项目（2024ZC07）。

详细信息

作者简介:
黄梓宸（1991-），广东省计量科学研究院工程师，研究方向：化学计量、碳计量、标准物质研究，邮箱：hzc@scm.com.cn

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出版历程
- 收稿日期: 2024-08-28
- 录用日期: 2024-11-01
- 修回日期: 2024-11-12
- 网络出版日期: 2024-11-21

Research on the Method for Reproducing Halogen Leak Rate Based on Reference Material

HUANG Zichen^{1, 2
,},
YIN Qiang¹,
YE Lifang¹,
JIA Xiangrui¹,
CHEN Ling^{1, 2},
ZHOU Junhong^{1, 2}

1.
Guangdong Provincial Institute of Metrology, Guangzhou 510405, China
2.
National Center for Carbon Metrology (Guangdong), Guangzhou 510405, China)

摘要

摘要: 卤素检漏仪校准所使用的标准漏孔一直以来存在不确定度较大的问题。为了降低卤素漏率量值的不确定度，提出了基于气体标准物质的漏率量值复现方法。经公式推导得到了在特定条件下气体浓度与漏率的转换关系，并通过实验进行了验证。结果表明使用卤素检漏仪测量复现漏率与标准漏孔漏率的一致性良好（两组实验归一化偏差为0.41及0.21）。分析了标准物质复现漏率的不确定度来源，包括气体标准物质、吸入流量、温度、压力等，计算并合成各分量，最终得到基于气体标准物质的复现漏率相对扩展不确定度为2.5%（k=2），证明使用气体标准物质进行漏率复现的不确定度水平显著低于常见标准漏孔，同时还具有良好的可操作性。
- 计量学 /
- 气体标准物质 /
- 卤素标准漏孔 /
- 漏率 /
- 不确定度
Abstract: The reference leak used for calibration of halogen leak detectors has always had a high degree of uncertainty. In order to reduce the uncertainty of halogen leak rate values, a method for reproducing leak rate based on gas reference material was proposed. The conversion relationship between gas concentration and leak rate under specific conditions was obtained through formula derivation and verified through experiments. The results showed that the consistency between the reproduced leak rate and the standard leak rate measured by halogen leak detector was excellent (the normalized deviations of the two experiments were 0.41 and 0.21). The components of uncertainty of the reproduced leak rate were analyzed, including gas reference material, inhale flow, temperature, pressure, molar mass and gas constant. After calculation and synthesis, the relative expanded uncertainty of the reproduction leakage rate based on gas reference material was obtained as 2.5% (k=2), which is significantly lower than that of common reference leak, also the method has good operability.
- metrology /
- gas reference material /
- halogen reference leak /
- leak rate /
- uncertainty

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图 1 装置连接示意图

Figure 1. Schematic diagram of instrument connection

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图 2 漏率测量结果

Figure 2. Measurement results of leak rate

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图 3 不确定度来源分析

Figure 3. Analysis of uncertainty sources

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表 1 检漏仪吸入流量测量结果

Table 1. Measurement results of leak detector inhale flow

测量次数	测量结果 / (mL·min⁻¹)	测量次数	测量结果 / (mL·min⁻¹)
1	59.2	6	59.6
2	59.0	7	59.4
3	59.6	8	59.8
4	58.9	9	60.5
5	59.6	10	59.6

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表 2 实验结果汇总

Table 2. Summary of experimental results

测量对象	标准值/ (g·a⁻¹)	实测值/ (g·a⁻¹)	标准偏差/ (g·a⁻¹)	示值误差/ (g·a⁻¹)
漏孔1	3.57	3.6	0.074	+0.03
标气1	3.86	3.8	0.052	−0.06
漏孔2	10.76	10.8	0.103	+0.04
标气2	10.93	11.1	0.063	+0.17

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表 3 测量不确定度计算结果

Table 3. Calculation results of measurement uncertainty

测量对象	u_漏率/ (g·a⁻¹)	u_重复性/ (g·a⁻¹)	u_分辨力/ (g·a⁻¹)	u_测量/ (g·a⁻¹)
漏孔1	0.089	0.023	0.029	0.094
标气1	0.048	0.016	0.029	0.056
漏孔2	0.269	0.033	0.029	0.271
标气2	0.137	0.020	0.029	0.140

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表 4 归一化偏差计算结果

Table 4. Calculation results of normalized deviation

测量对象	示值误差/ (g·a⁻¹)	u_测量/ (g·a⁻¹)	U_测量/ (g·a⁻¹)	E_n
漏孔1	+0.03	0.094	0.19	0.41
标气1	−0.06	0.056	0.11	0.41
漏孔2	+0.04	0.271	0.54	0.21
标气2	+0.17	0.140	0.28	0.21

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